Reaktionsgleichung
[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[NH:11][N:12]=[C:13]([C:20](=[O:22])[CH3:21])[CH2:14][C:15](OCC)=[O:16])[C:5]([OH:7])=[O:6].C(O)C.C(=O)([O-])[O-].[Na+].[Na+].Cl>O>[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[N:11]1[C:15](=[O:16])[CH2:14][C:13]([C:20](=[O:22])[CH3:21])=[N:12]1)[C:5]([OH:7])=[O:6]Komponenten
6
Versuchsvorschrift
To a solution of a 5 g. (34 mmoles) of 3-methyl-4-[N′-(2-ethoxycarbonyl-1-acetylethylidene)hydrazino]benzoic acid in 25 ml. of ethanol and 25 ml. of water was added with stirring 34.3 ml. of a 1 M sodium carbonate solution. The mixture was stirred at room temperature for 24 hours. The resulting mixture was acidified to pH 3 with 6 M hydrochloric acid and the resulting solid was collected by filtration, washed with water and dried. The 3-methyl-4-(3-acetyl-5-oxo-2-pyrazolin-1-yl)benzoic acid has melting point of >250° C.
Aufarbeitung
- stirringThe mixture was stirred at room temperature for 24 hours
- filtrationthe resulting solid was collected by filtration
- washwashed with water
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-d1df5cda31824a5d94bced5112eb8bbb
- Quelldatensatz
- uspto-grants-2001_08
- Patentnummer
- US06271373B1
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